Preparation method of bi-component functional master batch and fiber of graphene quantum dots

Abstract

The invention belongs to the field of efficient dispersion and spinning, particularly relates to a preparation method of bi-component functional master batches and fibers of graphene and graphene quantum dots with the size smaller than 10 nanometers, and aims at solving the problems that in the prior art, materials are difficult to uniformly mix when being mixed, and in the mixing process, the materials cannot be uniformly mixed. In order to overcome the defect that a material cannot be heated at a constant temperature in the prior art, the invention provides the following scheme: the material comprises the following material components: 5-15 parts of physical method graphene within 500nm; 2-10 parts of graphene quantum dots within 10nm; 60-80 parts of a polymer matrix; aiming at effective dispersion of physical method graphene within 500nm and graphene quantum dots within 10nm in a matrix (such as PET, PA6, PP and the like) and application of the graphene quantum dots in a spinning process, uniform dispersion of a bi-component material in the matrix is realized through an innovative dispersion method, equipment improvement and a spinning process, and a high-performance composite fiber material is successfully prepared.

Description

Technical Field

[0001] The invention relates to the technical field of efficient dispersion and spinning, and in particular to a preparation method of a two-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers and a fiber. Background Art

[0002] Graphene and graphene oxide have excellent antibacterial properties. The mechanism of graphene oxide sterilization / deodorization is that when it comes into contact with bacteria, the cell membrane is under pressure, and due to the mutual oxidation between its oxidized functional groups and the membrane, the bacteria are pierced and ruptured, and the RNA or DNA in the bacterial cells flows out and is inactivated. In addition, the addition of graphene oxide has a large specific surface area, which can be as high as 500 to 1000m2 / g, and has a very strong adsorption capacity. It has an excellent adsorption and removal effect on odors. It has excellent biocompatibility, toxicity, environmental protection, and safety. It is one of the antibacterial and deodorizing materials with great application potential.

[0003] At present, there is a technical problem of poor preparation of two-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers, and when making masterbatch of graphene quantum dots, when physical method graphene within 500nm and graphene quantum dots within 10nm are mixed in a matrix (PET, PA6 and PP materials, etc.), the mixing device used is difficult to achieve uniform mixing; and when physical method graphene within 500nm and graphene quantum dots within 10nm are mixed in a matrix (PET, PA6 and PP materials, etc.), it is difficult to maintain a constant temperature, which makes it easy to have corresponding quality problems when making two-component functional masterbatch. In view of the above problems, the present invention document proposes a preparation method of two-component functional masterbatch and fiber of graphene plus graphene quantum dots below 10 nanometers. Summary of the invention

[0004] The invention provides a preparation method of a double-component functional masterbatch of graphene plus graphene quantum dots with a size less than 10 nanometers and a fiber, which solves the shortcomings existing in the prior art.

[0005] The present invention provides the following technical solutions: A method for preparing a dual-component functional masterbatch of graphene and graphene quantum dots with a diameter of less than 10 nanometers, comprising the following steps: S1: Premix physical graphene within 500nm and graphene quantum dots within 10nm according to the proportion; S2: putting the product obtained by mixing in step S1, the polymer matrix and the dispersant into a mixer for mixing to obtain modified graphene quantum dots; S3: The modified graphene quantum dots obtained in step S2 are placed into a granulator to produce dual-component functional masterbatches.

[0006] As a further improvement of the above technical solution: The mixer includes a base frame, a processing box is fixedly installed on the top of the base frame, a plurality of electric push rods are fixedly installed at equal intervals on the outside of the processing box, a same cover plate is fixedly installed on the output shafts of the plurality of electric push rods, the cover plate is clamped with the top opening of the processing box, a double-layer mixing box is fixedly installed in the processing box, and further includes: A filling mechanism, which is installed on the top of the cover plate and is used to fill materials and solvents; A mixing mechanism, which is installed on the filling mechanism, and the bottom of the mixing mechanism extends into the double-layer mixing box. The mixing mechanism is used to mix and stir the materials evenly; A heating medium conveying mechanism, the heating medium conveying mechanism is installed on the bottom inner wall of the processing box, and the top of the heating medium conveying mechanism extends into the double-layer mixing box and is connected to the inner wall of the interlayer of the double-layer mixing box; Multiple heating mechanisms are installed at equal intervals on the outside of the processing box, the top of the heating mechanism extends into the interlayer of the double-layer mixing box, and the bottom of the heating mechanism extends into the processing box. The heating mechanism is used to circulate and heat the heating medium.

[0007] The filling mechanism includes a material filling box fixedly installed on the top of the cover plate, a push plate is slidably connected in the material filling box, an arc-shaped push rod is fixedly installed on one side of the push plate, one end of the arc-shaped push rod extends to the outside of the material filling box, a connecting box is fixedly installed through the cover plate, a mixing mechanism passes through the connecting box and is connected to the connecting box, a conveying pipe is fixedly installed on an inner wall of one side of the connecting box, one end of the conveying pipe extends into the material filling box and is fixedly connected to an inner wall of one side of the material filling box, a mixture injection pipe is fixedly installed through the inner wall of the top of the conveying pipe, a filling pipe is fixedly installed on the inner wall of one side of the top of the material filling box, the top of the filling pipe extends to the top of the material filling box, a sealing cap is clamped in the filling pipe, a power assembly is installed on the top of the cover plate, and the power assembly is respectively connected to the connecting box and the arc-shaped push rod.

[0008] The power assembly includes a mounting frame fixedly installed on the top of the cover plate, a stepper motor is fixedly installed on the top of the mounting frame, the output shaft of the stepper motor extends into the mounting frame and is fixedly installed with a driving gear, a mounting ring is provided on a rotating sleeve on the connecting box, an arc-shaped rack is fixedly installed on the mounting ring, the driving gear is meshed with the arc-shaped rack, a transmission rod is fixedly installed on the mounting ring, and the transmission rod is fixedly connected to the arc-shaped push rod.

[0009] A fixing seat is fixedly installed in the conveying pipe, a conical hole is opened on the fixing seat, a mounting plate is fixedly installed in the conical hole, a limiting rod is slidably connected through the mounting plate, a spherical plate is fixedly installed at one end of the limiting rod, the spherical plate is used to block the conical hole, a compression spring is sleeved on the limiting rod, and two ends of the compression spring are respectively fixedly connected to one side of the mounting plate and the other end of the limiting rod.

[0010] The mixing mechanism includes a stirring motor fixedly installed on the top of the connecting box, the output shaft of the stirring motor extends into the connecting box and is fixedly installed with a rotating shaft, a support tube is fixedly installed on the bottom of the cover plate, the bottom end of the support tube extends into the double-layer stirring box, the bottom end of the rotating shaft penetrates the support tube and extends into the double-layer stirring box, a spiral conveying blade located in the support tube is fixedly sleeved on the rotating shaft, a support frame is fixedly installed on the bottom end of the rotating shaft, the support frame contacts the inner wall of the double-layer stirring box, two reciprocating screws are symmetrically rotatably connected to the top of the support frame, a stirring frame is arranged in the double-layer stirring box, two nuts are symmetrically fixedly installed on the top of the stirring frame, the reciprocating screws respectively penetrate the stirring frame and the nuts and are threadedly connected to the nuts, a transmission gear is fixedly installed on the top of the reciprocating screw, a fixing ring is fixedly installed on the bottom of the cover plate, a gear ring is fixedly sleeved on the fixing ring, and two transmission gears are meshed with the gear ring.

[0011] The heating medium conveying mechanism includes a power box fixedly installed on the inner wall of the bottom of the processing box, and a suction pipe and an output pipe are fixedly installed on the inner walls on both sides of the power box respectively. One end of the suction pipe and the top end of the output pipe extend into the processing box, and a diversion pipe is fixedly installed on the top end of the output pipe. A closed ring is fixedly installed in the interlayer of the double-layer mixing box, and both ends of the diversion pipe pass through the closed ring and are fixedly connected to the closed ring. A water pump motor is fixedly installed at the bottom of the processing box, and the output shaft of the water pump motor extends into the power box and is fixedly installed with turbine blades.

[0012] The heating mechanism includes a heat exchange tube fixedly installed on the processing box, the top and bottom ends of the heat exchange tube respectively extend into the interlayer of the double-layer mixing box and the inside of the processing box and are respectively fixedly connected to the inner wall of the interlayer of the double-layer mixing box and the inner wall of the bottom of one side of the processing box, a heating box located outside the processing box is fixedly sleeved on the heat exchange tube, a spiral electric heating tube is electrically connected in the heating box, and the heat exchange tube passes through the spiral electric heating tube.

[0013] A two-component functional masterbatch of graphene plus graphene quantum dots with a size of less than 10 nanometers is prepared by the above-mentioned preparation method of the two-component functional masterbatch of graphene plus graphene quantum dots with a size of less than 10 nanometers, and comprises the following material components: 5-15 parts of physical graphene within 500nm; 2-10 parts of graphene quantum dots within 10nm; 60-80 parts of polymer matrix; Dispersant 1-5 parts.

[0014] A method for preparing a fiber of graphene plus graphene quantum dots with a diameter of less than 10 nanometers, comprising the following steps: S1. The above-mentioned two-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers is mixed with a polymer masterbatch and a filler, and 2%-8% of the masterbatch protective agent is added during the spinning process; S2. Filament spinning: The mixed melt is fed into a spinning machine, cooled or solidified through a spinning sleeve to obtain continuous filaments. During the spinning process, the spinning temperature and the side blowing speed are controlled to obtain fibers with a spinning fineness of less than 0.5Dex; Staple fiber spinning: After the spinning fluid is extruded from the spinneret, it is cut into short segments of several centimeters to tens of centimeters by a cutting device to obtain short fibers.

[0015] It is to be understood that the foregoing general description and the following detailed description are exemplary only and are not restrictive of the invention.

[0016] Compared with the prior art, the beneficial effects of the present invention are as follows: in the present invention, the filling mechanism is provided, and the arc-shaped push rod can be driven to move by starting the power assembly, and at this time, the material in the material filling box can be transported to the connecting box through the conveying pipe, and then transported to the double-layer mixing box by the connecting box, and at the same time, the mixture used to promote the fusion of the materials can be filled into the conveying pipe through the mixture injection pipe, so that it can be transported into the double-layer mixing box along with the materials; In the present invention, by means of the provided mixing mechanism, the rotating shaft can be driven to rotate by starting the stirring motor, and at this time, the spiral conveying blade can be driven to rotate, and the materials and the mixture entering the connecting box can fall downward, and at this time, the rotating spiral conveying blade can convey the materials, so that the materials enter the double-layer stirring box, and when the rotating shaft rotates, it can drive the supporting frame to rotate, and at this time, it can drive the two reciprocating screws to perform circular motion, and when the transmission gear performs circular motion with the reciprocating screw, the reciprocating screw can be self-rotated under the meshing transmission action with the gear ring, so that the stirring frame can be driven to perform longitudinal reciprocating motion under the threaded transmission action with the nut, so that the materials can be evenly mixed and stirred; In the present invention, the heating medium conveying mechanism is set up, and the turbine blades can be driven to rotate by starting the water pump motor. At this time, the heating medium in the processing box can be sucked into the power box through the suction pipe by the principle of suction, and then can be conveyed to the shunt pipe through the output pipe. After conveying through the shunt pipe, the heating medium can be conveyed to the interlayer of the double-layer mixing box, so that the double-layer mixing box can be heated in all directions. In this way, when the materials are mixed and stirred, the temperature can be kept stable at all times, and the problem of unbalanced stability in the double-layer mixing box will not occur; In the present invention, by setting up a heating mechanism, when the liquid level of the heating medium in the interlayer of the double-layer stirring box is higher than the top of the heat exchange tube, the heating medium can flow back to the processing box through the heat exchange tube, and after the spiral electric heating tube is energized, the heat exchange tube can be heated. In this way, when the heating medium flows through the heat exchange tube, the heating medium can be heated so as to increase the temperature of the heating medium and enable the heating medium to heat the double-layer stirring box.

[0017] The present invention can achieve uniform mixing and stirring when mixing the product, polymer matrix, dispersant and mixing agent in step S2, and during the mixing and stirring process, the principle of heat exchange can be used to maintain a constant temperature in the double-layer mixing box, so that quality problems will not occur when the masterbatch is produced later. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 is a block diagram of the preparation method; Figure 2 This is a three-dimensional schematic diagram of the mixer structure from the first perspective; Figure 3 It is a three-dimensional schematic diagram of the mixer structure from the second perspective; Figure 4 It is a three-dimensional schematic diagram of the separation structure of the cover plate and the processing box in the mixer; Figure 5 This is a schematic diagram of the main cross-sectional structure of the mixer; Figure 6 It is a three-dimensional schematic diagram of the filling mechanism, mixing mechanism and cover plate connection structure in the mixer from a top view; Figure 7 It is a three-dimensional schematic diagram of the connection structure of the stepper motor, transmission gear, arc-shaped rack, mounting ring, transmission rod and arc-shaped push rod in the mixer; Figure 8 A bottom-up three-dimensional schematic diagram of a connection structure between a cover plate and a mixing mechanism in a mixer; Fig. 9 It is a three-dimensional schematic diagram of the structure of the heating medium conveying mechanism in the mixer; Fig.10 The fiber prepared in Example 2; Fig.11 The antibacterial performance test results of Example 2 are shown in FIG. Fig.12 The fiber prepared in Example 3; Fig.13 The antibacterial performance test results of Example 3 are shown in FIG.

[0019] Reference numerals: 1. Base frame; 2. Processing box; 3. Cover plate; 4. Material filling box; 5. Push plate; 6. Arc push rod; 7. Connection box; 8. Mounting ring; 9. Transmission rod; 10. Filling pipe; 11. Sealing cover; 12. Delivery pipe; 13. Mixing agent injection pipe; 14. Fixed seat; 15. Mounting plate; 16. Limiting rod; 17. Ball plate; 18. Double-layer mixing box; 19. Closing ring; 20. Power box; 21. Output pipe; 22. Diverter pipe; 23. Suction pipe; 24. Water pump Motor; 25. Turbine blades; 26. Heat exchange tubes; 27. Heating box; 28. Spiral electric heating tubes; 29. ​​Mounting frame; 30. Stepper motor; 31. Drive gear; 32. Arc rack; 33. Stirring motor; 34. Rotating shaft; 35. Spiral conveying blades; 36. Support tube; 37. Support frame; 38. Reciprocating screw; 39. Stirring frame; 40. Nut; 41. Fixing ring; 42. Gear ring; 43. Transmission gear; 44. Compression spring; 45. Electric push rod. DETAILED DESCRIPTION

[0020] The embodiments of the present invention are described below in conjunction with the accompanying drawings in the embodiments of the present invention.

[0021] In the description of the embodiments of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms, "connection" and "installation" should be understood in a broad sense. For example, "connection" can be a detachable connection or a non-detachable connection; it can be a direct connection or an indirect connection through an intermediate medium. In addition, "communication" can be a direct connection or an indirect connection through an intermediate medium, wherein "fixed" means that the two are connected to each other and the relative position relationship after the connection remains unchanged. The directional terms mentioned in the embodiments of the present invention, such as "inside", "outside", "top", "bottom", etc., are only reference to the directions of the drawings. Therefore, the directional terms used are for better and clearer explanation and understanding of the embodiments of the present invention, rather than indicating or implying that the referred device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the embodiments of the present invention.

[0022] Example 1: Reference Figure 1-13 A method for preparing a two-component functional masterbatch of graphene and graphene quantum dots below 10 nanometers includes the following steps and uses a specific mixer structure.

[0023] Material composition: Physical graphene within 500nm: 5-15 parts; Graphene quantum dots within 10nm: 2-10 parts; Polymer matrix: 60-80 parts; Dispersant: 1-5 parts.

[0024] Preparation method steps: Pre-mixing: Physical graphene within 500nm and graphene quantum dots within 10nm are pre-mixed in proportion to ensure that the two are evenly distributed.

[0025] Mixing in a blender: A specific mixer is used, which includes a base frame 1, a processing box 2 is fixedly installed on the top of the base frame 1, a plurality of electric push rods 45 are fixedly installed at equal intervals on the outside of the processing box 2, a same cover plate 3 is fixedly installed on the output shafts of the plurality of electric push rods 45, the cover plate 3 is clamped with the top opening of the processing box 2, and a double-layer mixing box 18 is fixedly installed in the processing box 2. The product obtained by mixing in step 1, the polymer matrix and the dispersant are placed in a double-layer stirring box 18 in the stirrer.

[0026] The mixer is started to mix the materials put in to obtain modified graphene quantum dots. During the mixing process, the mixing mechanism of the mixer mixes and stirs the materials evenly, and the heating mechanism circulates and heats the heating medium to provide a suitable mixing temperature.

[0027] Granulation in granulator: Putting the modified graphene quantum dots obtained in step 2 into a granulator; Through the processing of the granulator, a dual-component functional masterbatch is produced.

[0028] Mixer detailed structure and operation: Filling mechanism: includes a material filling box 4 fixedly installed on the top of the cover plate 3, a push plate 5 is slidably connected in the material filling box 4, an arc-shaped push rod 6 is fixedly installed on one side of the push plate 5, a connecting box 7 is fixedly installed on the cover plate 3, the mixing mechanism passes through the connecting box 7 and is connected to the connecting box 7, a conveying pipe 12 is fixedly installed on the inner wall of one side of the connecting box 7, one end of the conveying pipe 12 extends into the material filling box 4, a mixture injection pipe 13 is fixedly installed on the top inner wall of the conveying pipe 12, a filling pipe 10 is fixedly installed on the inner wall of one side of the top of the material filling box 4, the top end of the filling pipe 10 extends to the top of the material filling box 4, and a sealing cover 11 is clamped in the filling pipe 10.

[0029] Power assembly: includes a mounting frame 29 fixedly mounted on the top of the cover plate 3, a stepper motor 30 fixedly mounted on the top of the mounting frame 29, the output shaft of the stepper motor 30 extends into the mounting frame 29 and is fixedly mounted with a driving gear 31, a mounting ring 8 is rotatably sleeved on the connecting box 7, an arc-shaped rack 32 is fixedly mounted on the mounting ring 8, the driving gear 31 is meshed with the arc-shaped rack 32, a transmission rod 9 is fixedly mounted on the mounting ring 8, and the transmission rod 9 is fixedly connected to the arc-shaped push rod 6.

[0030] By starting the stepper motor 30, the driving gear 31 is driven to rotate. At this time, under the meshing transmission action with the arc-shaped rack 32, the mounting ring 8 can be driven to rotate, thereby driving the transmission rod 9 to swing, thereby pushing the arc-shaped push rod 6 to move. In this way, the material in the material filling box 4 is transported to the connecting box 7 through the conveying pipe 12, and is transported to the double-layer mixing box 18 by the connecting box 7. At the same time, the mixture used to promote the fusion of the materials can be added to the conveying pipe 12 by the mixture injection pipe 13, and enters the double-layer mixing box 18 along with the material transportation.

[0031] A fixing seat 14 is fixedly installed in the conveying pipe 12, and a conical hole is opened on the fixing seat 14. A mounting plate 15 is fixedly installed in the conical hole, and a limiting rod 16 is slidably connected through the mounting plate 15. A spherical plate 17 is fixedly installed at one end of the limiting rod 16. The function of the spherical plate 17 is to block the conical hole. A compression spring 44 is also sleeved on the limiting rod 16, and the two ends of the spring are fixedly connected to one side of the mounting plate 15 and the other end of the limiting rod 16 respectively.

[0032] When there is no need to add material, the spherical plate 17 will block the tapered hole to prevent the mixture from flowing into the material filling box 4. When the material is pushed to the conveying pipe 12, the material will generate a thrust on the spherical plate 17, causing it to move and open the tapered hole to allow the material to pass through. While the spherical plate 17 moves, it will also drive the limiting rod 16 to move and compress the compression spring 44. Once the material filling stops, the compression spring 44 in a stressed state will drive the limiting rod 16 to move in the opposite direction, causing the spherical plate 17 to block the tapered hole again.

[0033] The structure and operation of the mixing mechanism: The mixing mechanism includes a stirring motor 33 fixedly mounted on the top of the connecting box 7, the output shaft of the stirring motor 33 extends into the connecting box 7, and a rotating shaft 34 is fixedly mounted thereon, a supporting tube 36 is fixedly mounted at the bottom of the cover plate 3, the bottom end of the supporting tube 36 extends into the double-layer stirring box 18, the bottom end of the rotating shaft 34 passes through the supporting tube 36 and extends into the double-layer stirring box 18, and a spiral conveying blade 35 located in the supporting tube 36 is fixedly mounted thereon.

[0034] A support frame 37 is also fixedly installed at the bottom end of the rotating shaft 34, and the support frame 37 is in contact with the inner wall of the double-layer mixing box 18. Two reciprocating screws 38 are symmetrically rotatably connected to the top of the support frame 37. A stirring frame 39 is arranged in the double-layer mixing box 18, and two nuts 40 are symmetrically fixedly installed on the top of the stirring frame 39. The reciprocating screws 38 respectively penetrate the stirring frame 39 and the nuts 40 and are threadedly connected to the nuts 40.

[0035] A transmission gear 43 is fixedly mounted on the top of the reciprocating screw 38 , and a fixing ring 41 is fixedly mounted on the bottom of the cover plate 3 . A gear ring 42 is fixedly sleeved on the fixing ring 41 , and both transmission gears 43 are meshed with the gear ring 42 .

[0036] When the stirring motor 33 is started, it will drive the rotating shaft 34 to rotate, and then drive the spiral conveying blades 35 to rotate. The materials and mixtures entering the connecting box 7 will fall downward and be transported to the double-layer stirring box 18 by the rotating spiral conveying blades 35. At the same time, the rotating rotating shaft 34 will also drive the supporting frame 37 to rotate, and then drive the two reciprocating screws 38 to perform circular motion. Under the meshing transmission action of the transmission gear 43 and the gear ring 42, the reciprocating screw 38 will rotate on its own, and drive the stirring frame 39 to perform longitudinal reciprocating motion through the threaded transmission action with the nut 40, thereby achieving uniform mixing and stirring of the materials.

[0037] The structure and operation of the heating medium conveying mechanism: The heating medium conveying mechanism includes a power box 20 fixedly mounted on the inner wall at the bottom of the processing box 2, and a suction pipe 23 and an output pipe 21 are fixedly mounted on the inner walls on both sides of the power box 20, one end of the suction pipe 23 and the top end of the output pipe 21 extend into the processing box 2, and a shunt pipe 22 is fixedly mounted on the top end of the output pipe 21.

[0038] A closed ring 19 is fixedly installed in the interlayer of the double-layer mixing box 18, and both ends of the diversion pipe 22 pass through the closed ring 19 and are fixedly connected thereto. A water pump motor 24 is also fixedly installed at the bottom of the processing box 2. The output shaft of the water pump motor 24 extends into the power box 20 and is fixedly installed with a turbine blade 25.

[0039] When the water pump motor 24 is started, it will drive the turbine blades 25 to rotate. Using the principle of suction, the heating medium in the processing box 2 will be sucked into the power box 20, and then transported to the diversion pipe 22 through the output pipe 21. After being transported by the diversion pipe 22, the heating medium will be transported to the interlayer of the double-layer mixing box 18, thereby heating the double-layer mixing box 18 in all directions. In this way, the temperature can be kept stable when the materials are mixed and stirred, avoiding the problem of temperature imbalance.

[0040] The structure and operation of the heating mechanism: The heating mechanism includes a heat exchange tube 26 fixedly mounted on the processing box 2, the top and bottom ends of the heat exchange tube 26 respectively extend into the interlayer of the double-layer mixing box 18 and the processing box 2, and are respectively fixedly connected to the inner wall of the interlayer of the double-layer mixing box 18 and the inner wall of the bottom of one side of the processing box 2, a heating box 27 located on the outside of the processing box 2 is fixedly mounted on the heat exchange tube 26, and a spiral electric heating tube 28 is electrically connected in the heating box 27, and the heat exchange tube 26 passes through the spiral electric heating tube 28.

[0041] When the liquid level of the heating medium in the interlayer of the double-layer stirring box 18 is higher than the top of the heat exchange tube 26, the heating medium will flow back to the processing box 2 through the heat exchange tube 26. After the spiral electric heating tube 28 is energized, it will heat the heat exchange tube 26. In this way, when the heating medium flows through the heat exchange tube 26, it will be heated, thereby increasing the temperature of the heating medium so that it can heat the double-layer stirring box 18 more effectively.

[0042] A method for preparing a fiber of graphene plus graphene quantum dots with a diameter of less than 10 nanometers, comprising the following steps: S1. The above-mentioned two-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers is mixed with a polymer masterbatch and a filler, and 2%-8% of the masterbatch protective agent is added during the spinning process; S2. Filament spinning: The mixed melt is fed into a spinning machine, cooled or solidified through a spinning sleeve to obtain continuous filaments. During the spinning process, the spinning temperature and the side blowing speed are controlled to obtain fibers with a spinning fineness of less than 0.5Dex; Staple fiber spinning: After the spinning fluid is extruded from the spinneret, it is cut into short segments of several centimeters to tens of centimeters by a cutting device to obtain short fibers.

[0043] Working principle: first, after cleaning the inner wall of the double-layer mixing box 18, the four electric push rods 45 can be started to drive the cover plate 3 to move downward, so that the cover plate 3 is engaged with the processing box 2, and then the pre-mixed physical graphene within 500nm and graphene quantum dots within 10nm, polymer matrix and dispersant are injected into the material filling box 4 through the filling pipe 10, and the mixture injection pipe 13 is connected to the external mixture filling pipeline. Then the stepper motor 30 can be started to drive the drive gear 31 to rotate. At this time, under the meshing transmission action with the arc-shaped rack 32, the mounting ring 8 can be driven to rotate, so that the transmission rod 9 can be driven to swing, thereby pushing the arc-shaped push rod 6 to move, and at this time, it can be The material in the material filling box is conveyed to the connecting box 7 through the conveying pipe 12, and then conveyed to the double-layer mixing box 18 by the connecting box 7. At the same time, the mixture used to promote the fusion of the materials can be injected into the conveying pipe 12 through the mixture injection pipe 13, so that the materials can be conveyed into the double-layer mixing box 18. When the materials are pushed into the conveying pipe 12, the materials exert a thrust on the spherical plate 17 to move it, so that the conical hole can be opened to facilitate the movement of the materials. At the same time, when the spherical plate 17 moves, it can drive the limiting rod 16 to move and compress the compression spring 44. The compression spring 44 in a stressed state can drive the limiting rod 16 to reset in the opposite direction when no materials are added, so that the limiting rod 16 can be used. The spherical plate 17 keeps the tapered hole blocked. At the same time, when the material enters the conveying pipe 12, the mixture can also be injected into the conveying pipe 12. At this time, under the flushing of the mixture, the material can enter the connecting box 7. Then the stirring motor 33 is started to drive the rotating shaft 34 to rotate. At this time, the spiral conveying blade 35 can be driven to rotate, and the material and the mixture entering the connecting box 7 can fall downward. At this time, the rotating spiral conveying blade 35 can convey the material, so that the material enters the double-layer mixing box 18, and when the rotating shaft 34 rotates, it can drive the support frame 37 to rotate. At this time, it can drive the two reciprocating screws 38 to perform annular motion. When the transmission gear 43 performs annular motion with the reciprocating screw 38, it can be rotated with the gear ring 42 Under the action of meshing transmission, the reciprocating screw 38 can rotate on its own, so that under the action of the threaded transmission with the nut 40, the stirring frame 39 can be driven to perform longitudinal reciprocating motion, so that the materials can be evenly mixed and stirred. At the same time, the water pump motor 24 can be started to drive the turbine blades 25 to rotate. At this time, the heating medium in the processing box 2 can be sucked into the power box 20 through the suction pipe 23 by the principle of suction, and then can be transported to the diverter pipe 22 through the output pipe 21. After being transported by the diverter pipe 22, the heating medium can be transported to the interlayer of the double-layer stirring box 18. When the liquid level of the heating medium in the interlayer of the double-layer stirring box 18 is higher than the top of the heat exchange tube 26, the heating medium and the heat exchange tube 26 flow back to the processing box 2.After the spiral electric heating tube 28 is energized, the heat exchange tube 26 can be heated. When the heating medium flows through the heat exchange tube 26, the heating medium can be heated to increase the temperature of the heating medium, so that the heating medium can heat the double-layer mixing box 18. When the heating medium fills the interlayer of the double-layer mixing box 18, the double-layer mixing box 18 can be heated in all directions. When the materials are mixed and stirred, the temperature can be kept stable at all times, and there will be no problem of uneven stability in the double-layer mixing box 18.

[0044] Example 2: Physical method graphene within 500nm: 10 parts; Graphene quantum dots within 10nm: 8 parts; Polymer matrix: 80 parts; Dispersant: 2 parts of masterbatch prepared in the ratio of 1 to 2 parts.

[0045] Example 3: Physical method graphene within 500nm: 12 parts; Graphene quantum dots within 10nm: 10 parts; Polymer matrix: 75 parts; Dispersant: 3 parts of masterbatch prepared in the ratio of fiber material.

[0046] The above are only specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can easily think of changes or substitutions within the technical scope disclosed by the present invention, which should be included in the protection scope of the present invention. In the absence of conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other. Therefore, the protection scope of the present invention should be based on the protection scope of the claims.

Claims

1. A method for preparing a two-component functional masterbatch of graphene and graphene quantum dots below 10 nanometers, characterized in that: The following steps are involved: S1: Premix physical graphene within 500nm and graphene quantum dots within 10nm according to the proportion; S2: putting the product obtained by mixing in step S1, the polymer matrix and the dispersant into a mixer for mixing to obtain modified graphene quantum dots; S3: The modified graphene quantum dots obtained in step S2 are placed into a granulator to produce dual-component functional masterbatches.

2. The method for preparing a dual-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers according to claim 1, characterized in that: The mixer comprises a base frame (1), a processing box (2) is fixedly mounted on the top of the base frame (1), a plurality of electric push rods (45) are fixedly mounted at equal intervals on the outside of the processing box (2), a same cover plate (3) is fixedly mounted on the output shafts of the plurality of electric push rods (45), the cover plate (3) is clamped with the top opening of the processing box (2), a double-layer mixing box (18) is fixedly mounted in the processing box (2), and further comprises: A filling mechanism, which is installed on the top of the cover plate (3) and is used to fill materials and solvents; A mixing mechanism, the mixing mechanism is mounted on the filling mechanism, the bottom of the mixing mechanism extends into the double-layer mixing box (18), and the mixing mechanism is used to evenly mix and stir the materials; A heating medium conveying mechanism, the heating medium conveying mechanism being mounted on the bottom inner wall of the processing box (2), the top of the heating medium conveying mechanism extending into the double-layer stirring box (18) and connected to the inner wall of the interlayer of the double-layer stirring box (18); A plurality of heating mechanisms are installed at equal intervals on the outside of the processing box (2), the top of the heating mechanism extends into the interlayer of the double-layer stirring box (18), and the bottom of the heating mechanism extends into the processing box (2), and the heating mechanism is used to circulate and heat the heating medium.

3. The method for preparing a dual-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers according to claim 2, characterized in that: The filling mechanism comprises a material filling box (4) fixedly mounted on the top of the cover plate (3), a push plate (5) slidably connected inside the material filling box (4), an arc-shaped push rod (6) fixedly mounted on one side of the push plate (5), one end of the arc-shaped push rod (6) extending to the outside of the material filling box (4), a connecting box (7) passing through and fixedly mounted on the cover plate (3), the mixing mechanism passing through the connecting box (7) and connected to the connecting box (7), a conveying pipe (12) fixedly mounted on the inner wall of one side of the connecting box (7), one end of the conveying pipe (12) The conveying pipe (12) extends into the material filling box (4) and is fixedly connected to an inner wall of one side of the material filling box (4); a mixture injection pipe (13) is fixedly installed on the inner wall of the top of the conveying pipe (12); a filling pipe (10) is fixedly installed on the inner wall of one side of the top of the material filling box (4); the top end of the filling pipe (10) extends to the top of the material filling box (4); a sealing cover (11) is clamped in the filling pipe (10); a power assembly is installed on the top of the cover plate (3); and the power assembly is respectively connected to the connection box (7) and the arc-shaped push rod (6).

4. The method for preparing a dual-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers according to claim 3, characterized in that: The power assembly comprises a mounting frame (29) fixedly mounted on the top of the cover plate (3); a stepper motor (30) is fixedly mounted on the top of the mounting frame (29); an output shaft of the stepper motor (30) extends into the mounting frame (29) and is fixedly mounted with a driving gear (31); a mounting ring (8) is rotatably sleeved on the connection box (7); an arc-shaped rack (32) is fixedly mounted on the mounting ring (8); the driving gear (31) is meshed with the arc-shaped rack (32); a transmission rod (9) is fixedly mounted on the mounting ring (8); and the transmission rod (9) is fixedly connected to the arc-shaped push rod (6).

5. The method for preparing a dual-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers according to claim 4, characterized in that: A fixing seat (14) is fixedly installed in the delivery pipe (12), a tapered hole is formed on the fixing seat (14), a mounting plate (15) is fixedly installed in the tapered hole, a limiting rod (16) is slidably connected to the mounting plate (15), a spherical plate (17) is fixedly installed at one end of the limiting rod (16), and the spherical plate (17) is used to block the tapered hole, and a compression spring (44) is sleeved on the limiting rod (16), and two ends of the compression spring (44) are respectively fixedly connected to one side of the mounting plate (15) and the other end of the limiting rod (16).

6. The method for preparing a dual-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers according to claim 5, characterized in that: The mixing mechanism comprises a stirring motor (33) fixedly mounted on the top of the connection box (7); the output shaft of the stirring motor (33) extends into the connection box (7) and is fixedly mounted with a rotating shaft (34); a support tube (36) is fixedly mounted on the bottom of the cover plate (3); the bottom end of the support tube (36) extends into the double-layer stirring box (18); the bottom end of the rotating shaft (34) passes through the support tube (36) and extends into the double-layer stirring box (18); a spiral conveying blade (35) located in the support tube (36) is fixedly sleeved on the rotating shaft (34); a support frame (37) is fixedly mounted on the bottom end of the rotating shaft (34); the support frame (37) and the double-layer stirring box are connected to each other. The inner wall of the cover plate (18) is in contact with each other, the top of the support frame (37) is symmetrically rotatably connected with two reciprocating screws (38), a stirring frame (39) is arranged in the double-layer stirring box (18), and two nuts (40) are symmetrically fixedly installed on the top of the stirring frame (39), the reciprocating screws (38) respectively penetrate the stirring frame (39) and the nuts (40) and are threadedly connected with the nuts (40), a transmission gear (43) is fixedly installed on the top of the reciprocating screw (38), a fixing ring (41) is fixedly installed on the bottom of the cover plate (3), a gear ring (42) is fixedly sleeved on the fixing ring (41), and the two transmission gears (43) are meshed with the gear ring (42).

7. The method for preparing a dual-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers according to claim 6, characterized in that: The heating medium conveying mechanism comprises a power box (20) fixedly mounted on the inner wall at the bottom of the processing box (2), a suction pipe (23) and an output pipe (21) are fixedly mounted on the inner walls on both sides of the power box (20), one end of the suction pipe (23) and the top end of the output pipe (21) both extend into the processing box (2), a diverter pipe (22) is fixedly mounted on the top end of the output pipe (21), a closed ring (19) is fixedly mounted in the interlayer of the double-layer stirring box (18), both ends of the diverter pipe (22) penetrate the closed ring (19) and are fixedly connected to the closed ring (19), a water pump motor (24) is fixedly mounted on the bottom of the processing box (2), an output shaft of the water pump motor (24) extends into the power box (20) and is fixedly mounted with turbine blades (25).

8. The method for preparing a dual-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers according to claim 7, characterized in that: The heating mechanism comprises a heat exchange tube (26) fixedly mounted on the processing box (2), the top and bottom ends of the heat exchange tube (26) respectively extending into the inner layer of the double-layer stirring box (18) and the inner layer of the processing box (2) and respectively fixedly connected to the inner wall of the inner layer of the double-layer stirring box (18) and the inner wall of the bottom of one side of the processing box (2), a heating box (27) located outside the processing box (2) is fixedly sleeved on the heat exchange tube (26), a spiral electric heating tube (28) is electrically connected inside the heating box (27), and the heat exchange tube (26) passes through the spiral electric heating tube (28).

9. A two-component functional masterbatch of graphene plus graphene quantum dots with a size of less than 10 nanometers, prepared by the preparation method of the two-component functional masterbatch of graphene plus graphene quantum dots with a size of less than 10 nanometers as claimed in claim 8, characterized in that: Includes the following material components: 5-15 parts of physical graphene within 500nm; 2-10 parts of graphene quantum dots within 10nm; 60-80 parts of polymer matrix; Dispersant 1-5 parts.

10. A method for preparing a fiber of graphene plus graphene quantum dots with a diameter of less than 10 nanometers, characterized in that: The following steps are involved: S1. The two-component functional masterbatch of graphene plus graphene quantum dots below 10 nanometers as claimed in claim 9 is mixed with a polymer masterbatch and a filler, and 2%-8% of a masterbatch protective agent is added during the spinning process; S2. Filament spinning: The mixed melt is fed into a spinning machine, cooled or solidified through a spinning sleeve to obtain continuous filaments. During the spinning process, the spinning temperature and the side blowing speed are controlled to obtain fibers with a spinning fineness of less than 0.5Dex; Staple fiber spinning: After the spinning fluid is extruded from the spinneret, it is cut into short segments of several centimeters to tens of centimeters by a cutting device to obtain short fibers.

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